HCID 21914731、化合物 → HCID 21914837、化合物

HRID 2117868ノート

反応式

HRID 2117868 の反応式
[OH:1][CH2:2][C:3]1[N:4]=[C:5]([NH:8][C:9](=[O:13])[O:10][CH2:11][CH3:12])[S:6][CH:7]=1>C(Cl)(Cl)Cl.CO.[O-2].[Mn+4].[O-2]>[CH:2]([C:3]1[N:4]=[C:5]([NH:8][C:9](=[O:13])[O:10][CH2:11][CH3:12])[S:6][CH:7]=1)=[O:1]

参加物

5

反応物 1

HCID 21914731HCID 21914731、化合物

生成物 1

HCID 21914837HCID 21914837、化合物収率 106.4%

試薬・触媒・溶媒 3

HCID 178418406HCID 178418406、化合物触媒2 回HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

To a mixed solution of ethyl 4-(hydroxymethyl)-1,3-thiazol-2-ylcarbamate (446 mg) in chloroform (30 ml) and methanol (3 ml) was added portionwise manganese (IV) oxide chemicals treated (1.92 g) at room temperature. After the mixture was stirred at the same temperature for 2 hours, then treated manganese (IV) oxide chemicals (250 mg) was added again to the solution, and it was stirred at 50° C. for 3 hours. Manganese (IV) oxide was removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (10 g) using a mixed solvent of hexane and ethyl acetate (4:1). The fractions containing the objective compound were collected and evaporated under reduced pressure to give colorless powder (470 mg, 106.4%).

後処理

  1. additiontreated (1.92 g) at room temperature
  2. stirringwas stirred at 50° C. for 3 hours
  3. customManganese (IV) oxide was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by column chromatography on silica gel (10 g)
  6. additionThe fractions containing the objective compound
  7. customwere collected
  8. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-5228cc6187cc43fda3afe8c343c633aa
出典データセット
uspto-grants-2008_10
特許番号
US07442715B2

反応ノート

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